反应详情

To 2.28 g (10.0 mmole) of 3-trifluoromethyl-4-phenyl-5-aminoisoxazole were added 20 ml of conc. HCl and 1.09 g (11. 0 mmole) of cuprous chloride and 4.2 ml of aqueous sodium nitrate (2.76 g, 40 mmole) was added dropwise to the reaction mixture, keeping the temperature at 20°-25° C. After addition, the temperature was raised to 40°-45° C. and the mixture was stirred for 1 hour. To the mixture was added 16 ml of water, extracted with methylene chloride, dried with anhydrous sodium sulfate, evaporated under reduced pressure. The residue was purified by chromatography on silica gel to give 0.5651 g of colorless liquid. This was distilled under reduced pressure to give 0.4193 g of the titled compound as colorless liquid, yield 16.9%, b.p. 80.0°-83.0° C./0.50 mmHg.

1. additionwas added dropwise to the reaction mixture
2. customat 20°-25° C
3. additionAfter addition
4. temperaturethe temperature was raised to 40°-45° C.
5. extractionextracted with methylene chloride
6. dry with materialdried with anhydrous sodium sulfate
7. customevaporated under reduced pressure
8. customThe residue was purified by chromatography on silica gel